CN107611439A - A kind of preparation method of metal complex lithium ion battery electrode material - Google Patents
A kind of preparation method of metal complex lithium ion battery electrode material Download PDFInfo
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Abstract
A kind of preparation method of metal complex lithium ion battery electrode material, by Mg (NO3)2·6H2O, N, N bis- (5 M-phthalic acid) 1,4,5,8 benzene-naphthalene diimides in molar ratio 2:1 uniformly mixing, adds 30mL dimethylformamides（DMF）For solvent, 3mol/L hydrochloric acid, stirring at normal temperature are added；The mixture that preceding step obtains is entered into autoclave, 95 DEG C of constant temperature two days, cools down to obtain Mg NDI；Mg NDI complexs in preceding step are soaked into 24h in ethanol, are dried in vacuo after filtering, the metal complex activated；By the metal complex obtained in upper step and Kynoar, conductive black in mass ratio 60:10:30 configuration resulting mixtures, add solvent N methyl pyrrolidones, stir into sticky pulpous state electrode material；Re-coating is dried to obtain lithium ion battery electrode material on metal copper foil.
Description
Technical field
The present invention relates to a kind of preparation method of metal complex lithium ion battery electrode material.It is related to the acyl of magnesium-naphthalene two Asia
Amine（Abbreviation Mg-NDI）Technology of preparing as lithium ion battery negative material.
Background technology
Lithium ion battery, which is developed so far, to be widely used, the positive pole system of lithium ion battery in the market
It is still LiCoO2Layer structure type and its derivative, and LiFePO4Polyanionic and its derivative.Negative pole is still various
Carbon material.More mature and stable electrode material has its advantage at present, but shortcoming is also clearly.LiCoO2And ternary
The cyclical stability and security of layer structure material all have much room for improvement, while the cost of raw material is also higher.LiFePO4It is poly- cloudy from
Subtype and its derivative, energy density is small, poor performance at low temperatures.Therefore it is badly in need of developing new electrode system.Organic electrodes quilt
Think that future is possible to be widely used in lithium ion battery, organic electrodes have extraordinary oxidation-reduction pair, relatively low
Security risk, be easier the HOMO/LUMO energy levels of control, while organic matter has structured flexibility, can be size
Larger ion（102pm）Improve the passage of migration.Therefore the organic matter with oxidation-reduction pair is especially suitable for lithium-ion electric
Pond.Recent increasing researcher is by electrode system from inorganic to organic transformation；Research is found, contains C6 rings, structure
It is upper that there is carbonyl group can be combined with lithium ion.
The content of the invention
It is an object of the invention to provide a kind of metal complex lithium ion battery electrode material, to solve current lithium-ion electric
Insufficient problem present in the technology of pole.
Technical scheme：
A kind of preparation method of metal complex lithium ion battery electrode material, specifically includes following preparation process：
（1）By Mg (NO3)2·6H2O, N, N- bis- (5- M-phthalic acids) -1,4,5,8- benzene-naphthalene diimides in molar ratio 2:1 is uniform
Mixing, add 30mL dimethylformamides（DMF）For solvent, 3mol/L hydrochloric acid is added, stirring at normal temperature is no less than 30min；
（2）By step（1）Mixture after middle stirring is added in polytetrafluoroethylene (PTFE) autoclave, 95 DEG C of constant temperature two days；From
Room temperature so is cooled to, obtains yellowish-brown bulk crystals Mg-NDI；
（3）By step（2）In obtain yellowish-brown bulk crystals Mg-NDI complexs and soak 24h in ethanol, after filtering, not low
Vacuum drying is no more than 12h at 80 DEG C, removes the solvent molecule in complex hole, the metal complex Mg- activated
NDI；
（4）By step（3）In obtain metal complex Mg-NDI, Kynoar（PVDF）, conductive black Super-P is according to matter
Measure ratio 60:10:30 or 50:10:40 configuration resulting mixtures, add solvent N-methyl pyrilidone（NMP）, it is prepared into after stirring 2h
Sticky pulpous state electrode material；
（5）By step（4）In obtained sticky pulpous state electrode material, coated on metal copper foil, coating thickness is not more than 50 μm,
Under the conditions of drying temperature is not higher than 120 DEG C, drying time is not less than 6h, obtains lithium ion battery electrode material；
（6）By step（6）In obtained battery electrode material be cut into the circular pole piece that diameter meets the requirement of battery electrode size, gold
Category lithium piece is used as is to electrode, electrolyte：1mol/L LiPF6It is dissolved in ethylene carbonate（EC）And dimethyl carbonate（DMC）'s
In solvent（Mol ratio EC：DMC=1:1）, it is assembled into 2032 type button cells.
(the NO containing Mg3)2·6H2O, N, N- bis- (5- M-phthalic acids) -1,4,5,8- benzene-naphthalene diimides, dimethyl methyl
Acid amides（DMF）, it is that analysis is pure.
Mg (the NO3)2·6H2O is added in the reactor that 5~10mmol is 50~100mL to volume；N- bis- is (between 5-
Phthalic acid)-Isosorbide-5-Nitrae, 5,8- benzene-naphthalene diimides, add 2.5~5mmol；Concentration of hydrochloric acid is 3-6mol/L；Polytetrafluoroethyl-ne alkene reaction
Kettle product is 50~100mL.
Mg (the NO3)2·6H2The ratio of O, N, N- bis- (5- M-phthalic acids) -1,4,5,8- benzene-naphthalene diimides is according to rubbing
That ratio 2:1 progress is mixed uniformly.
The solvent is DMF, and addition is 30~60mL.
The step（5）Middle electrode slurry coating thickness is 30~50 μm.6~12h is dried at 100~120 DEG C.
The Kynoar（PVDF）, conductive black Super-P, 1-METHYLPYRROLIDONE（NMP）It is LITHIUM BATTERY.
The electrolyte is：1mol/L LiPF6It is dissolved in ethylene carbonate（EC）And dimethyl carbonate（DMC）Solvent
In（Mol ratio EC：DMC=1:1）.
The step（1）The molar concentration of middle hydrochloric acid is 36mol/L.
The step（1）Middle 30~60min of mixing time, stir speed (S.S.) are 200~500 r/min.
The step（2）Middle thermostat temperature is 90~100 DEG C, step（2）Middle constant temperature time is more than 24h.
The step（3）Middle ethanol exchange reaction, the ratio that ethanol adds is by ethanol weight than crystal weight 10~20:1
Ethanol soak time is 24h, is changed once every 6~8h, and exchange times are 3~4 times.
The step（3）In vacuum drying temperature be 80~100 DEG C, be dried in vacuo 10~12h.
The step（4）Middle complex Mg-NDI, PVDF, Super-P are according to mass ratio 60:10:30 or 50:10:40.
The amount that NMP is added is 3~4 times of complex Mg-NDI, PVDF, Super-P gross weight
Preferably, step（4）Middle metal complex Mg-NDI, Kynoar（PVDF）, conductive black Super-P quality
Than 60:10:30.
The step（4）Middle mixing time is 2h.
The step（5）Middle coating thickness is 50 μm.
Compared with prior art, the advantage of the invention is that：A kind of metal complex lithium ion battery electrode material magnesium-naphthalene
Imidodicarbonic diamide（Abbreviation Mg-NDI）.Metal complex Mg-NDi has structure novelty, and is to have report to be applied to lithium first
In ion battery electrode materials.The Mg-NDI metal complex materials, under 0.01V-3V, 20mA/g current density, first
Specific discharge capacity reaches 800mAh/g；2nd time circulation specific discharge capacity be 235mAh/g, discharge capacity after circulating for 20 times
140mAh/g.The present invention requires low to synthesis device, simple to operate.Synthesized new metal object complex Mg-NDI materials
Stability Analysis of Structures, it is cheap, it is environment-friendly, it is a kind of novel lithium ion battery electrode material.
Brief description of the drawings
Fig. 1 is the SEM spectrum of the product of the embodiment of the present invention 1.
Fig. 2 is the EDX collection of illustrative plates of the product of the embodiment of the present invention 1.
Fig. 3 is the first charge-discharge curve of the product of the embodiment of the present invention 1.
Fig. 4 is 20 charging and discharging curves of the product of the embodiment of the present invention 1.
Fig. 5 is the SEM spectrum of the product of the embodiment of the present invention 2.
Fig. 6 is the EDX collection of illustrative plates of the product of the embodiment of the present invention 2.
Fig. 7 is the first charge-discharge curve of the product of the embodiment of the present invention 2.
Fig. 8 is 20 charging and discharging curves of the product of the embodiment of the present invention 2.
Fig. 9 is the structure chart for the Mg-NDI electrode materials that the present invention synthesizes.
Embodiment
Technical scheme is illustrated as embodiment below in conjunction with Fig. 1,2,3,4.
Example 1, weigh 1.28 g（5mmol）Magnesium nitrate hexahydrate and 1.48g（2.5 mmol）N, (the 5- isophthalic two of N- bis-
Formic acid)-Isosorbide-5-Nitrae, 5,8- benzene-naphthalene diimides, 30ml DMF are added, then add 3mol/L hydrochloric acid 2ml, stirred under normal temperature
30min.Mixture after stirring is added in 50ml Teflon human relations autoclaves, and the reactor of good seal is put into an oven 95
DEG C constant temperature two days, then naturally cools to room temperature, obtains yellowish-brown bulk crystals.By the complex immersion of synthesis in ethanol
After 24h, filtering, 12h is dried in vacuo at 80 DEG C, removes the solvent molecule in complex hole, the complex Mg- activated
NDI.By ground 300 mesh sieves of dried Mg-NDI.By metal complex Mg-NDI, Kynoar（PVDF）, conductive charcoal
Black Super-P is according to mass ratio 60:10:30 configuration resulting mixtures, add solvent N-methyl pyrilidone（NMP）, after stirring 2h
It is prepared into sticky pulpous state electrode material.By sticky pulpous state electrode material, coated on metal copper foil, coating thickness is 50 μm,
12h is dried at 100 DEG C, obtains lithium ion cell electrode.Resulting battery electrode is cut into a diameter of 16mm circular pole piece, gold
Category lithium piece is used as is to electrode, electrolyte：1mol/L LiPF6It is dissolved in ethylene carbonate（EC）And dimethyl carbonate（DMC）'s
In solvent（Mol ratio EC：DMC=1:1）, 2032 type button cells are assembled into the glove box full of argon gas.
SEM morphology analysis and EDX energy spectrum analysis are carried out to synthesized Mg-NDI materials.SEM shown in Fig. 1 schemes, synthesized
Material granule be sheet aggregate.Fig. 2 is EDX energy spectrum analysis, as a result shows that element contained by sample is C, N, O, Mg, according to
Constituent content sxemiquantitative calculate sample in Mg stoichiometric proportion substantially close to（C75H35Mg4N13O32）, but C, N content are higher,
This is to still suffer from part DMF solvent molecule to be present in hole.The Mg-NDI positive electrodes that will be prepared, by m (Mg-NDI):
m(SP) :m ( PVDF) = 60:30:10, appropriate solvent NMP is added, is mixed, is applied on copper foil and positive pole is made；
Negative pole is metal lithium sheet；Electrolyte is 1 mol/L LiPF6/ EC+DMC (volume ratios 1:1), in the hand full of argon gas
2025 button cells are assembled into casing.Charge-discharge test is carried out to the button cell prepared.Test result such as Fig. 3 shows,
Under 20mA/g current density, first discharge specific capacity reaches 830mAhg-1.Fig. 4 is the charging and discharging curve after circulating first,
2nd circulation, the mAhg of discharge capacity 235-1, specific discharge capacity is 140 mAhg after 20 circulations-1。
Embodiment 2：5th, 6,7,8, weigh 1.28 g（5mmol）Magnesium nitrate hexahydrate and 1.48g（2.5 mmol）N, N-
Two (5- M-phthalic acids)-Isosorbide-5-Nitraes, 5,8- benzene-naphthalene diimides, 30ml DMF are added, then add 6mol/L hydrochloric acid 2ml,
60min is stirred under normal temperature.Mixture after stirring is added in 50ml Teflon human relations autoclaves, and the reactor of good seal is put
95 DEG C of constant temperature two days in an oven, then naturally cools to room temperature, obtains yellowish-brown bulk crystals.The complex of synthesis is soaked
In ethanol after 24h, filtering, 12h is dried in vacuo at 80 DEG C, removes the solvent molecule in complex hole, activated
Complex Mg-NDI2.By ground 300 mesh sieves of dried Mg-NDI2.By metal complex Mg-NDI, Kynoar
（PVDF）, conductive black Super-P is according to mass ratio 50:10:40 configuration resulting mixtures, add solvent N-methyl pyrilidone
（NMP）, electrode material viscous paste is prepared into after stirring 2h.By electrode material viscous paste, coated on metal copper foil, coat
Thickness is 50 μm, and 12h is dried at 100 DEG C, obtains lithium ion cell electrode.Resulting battery electrode is cut into a diameter of 16mm
Circular pole piece, metal lithium sheet as being to electrode, electrolyte：1mol/L LiPF6It is dissolved in ethylene carbonate（EC）And carbonic acid
Dimethyl ester（DMC）Solvent in（Mol ratio EC：DMC=1:1）, 2032 type buttons electricity is assembled into the glove box full of argon gas
Pond.
SEM morphology analysis and EDX energy spectrum analysis are carried out to synthesized Mg-NDI2 materials.SEM shown in Fig. 5 schemes, Mg-
It is larger second particle that NDI2 materials, which are reunited, and particle surface has many crackles.Fig. 6 is EDX energy spectrum analysis, as a result shows sample
Element contained by product is C, N, O, Mg, according to constituent content sxemiquantitative calculate the stoichiometric proportion of Mg in sample substantially close to
（C76H35Mg4N15O32）, C, N content are still higher, however it remains part DMF solvent molecule is present in hole.By what is prepared
Mg-NDI positive electrodes, by m (Mg-NDI2): m(SP) :m ( PVDF) = 50:40:10, add appropriate solvent
NMP, mixed, be applied on copper foil and positive pole is made；Negative pole is metal lithium sheet；Electrolyte is 1 mol/L LiPF6/ EC +
DMC (volume ratios 1:1) 2025 button cells, are assembled into the glove box full of argon gas.The button cell prepared is entered
Row charge-discharge test.Test result such as Fig. 7 shows that under 40mA/g current density, first discharge specific capacity reaches
821mAhg-1.Fig. 4 be first circulate after charging and discharging curve, the 2nd time circulation, the mAhg of discharge capacity 290-1, after 20 circulations
Specific discharge capacity is 150 mAhg-1。
Fig. 9 is the structure chart of the Mg-NDI electrode materials synthesized by the present invention, and benzene-naphthalene diimide is formed with metal Mg to be had
The complex of loose structure, lithium ion are combined with the carbonyl of benzene-naphthalene diimide, so as to receiving and losing electrons.
Mg-NDI electrode material discharge and recharge reaction procedure declarations prepared by the present invention, benzene-naphthalene diimide are gone back with lithium ion oxidation
Former reaction equation is as follows：
During electric discharge, Li+From negative pole by electrolyte, being combined with C=O in carbonyl, double bond becomes singly-bound, during charging, Li+From combination
Place's abjection, by electrolyte, returns to negative pole, C-O singly-bounds are changed into C=O double bonds again.
The Mg-NDI metal complex materials synthesized in the manner described above, under 0.01V-3V, 20mA/g current density,
First discharge specific capacity reaches 800mAh/g；2nd time circulation specific discharge capacity be 235mAh/g, discharge capacity after circulating for 20 times
140mAh/g.Low is required to synthesis device, it is simple to operate.Synthesized new metal object complex Mg-NDI material structures are steady
It is fixed, it is cheap, it is environment-friendly, it is a kind of novel anode material for lithium-ion batteries, there is preferable development prospect.
Claims (11)
1. a kind of preparation method of metal complex lithium ion battery electrode material, it is characterised in that specific make includes following step
Suddenly：
（1）By Mg (NO3)2·6H2O, N, N- bis- (5- M-phthalic acids) -1,4,5,8- benzene-naphthalene diimides in molar ratio 2:1 is uniform
Mixing, add 30mL dimethylformamides（DMF）For solvent, 3mol/L hydrochloric acid is added, stirring at normal temperature is no less than 30min；
（2）By step（1）Mixture after middle stirring is added in polytetrafluoroethylene (PTFE) autoclave, 95 DEG C of constant temperature two days；From
Room temperature so is cooled to, obtains yellowish-brown bulk crystals Mg-NDI；
（3）By step（2）In obtain yellowish-brown bulk crystals Mg-NDI complexs and soak 24h in ethanol, after filtering, not low
Vacuum drying is no more than 12h at 80 DEG C, removes the solvent molecule in complex hole, the metal complex Mg- activated
NDI；
（4）By step（3）In obtain metal complex Mg-NDI, Kynoar（PVDF）, conductive black Super-P is according to matter
Measure ratio 60:10:30 or 50:10:40 configuration resulting mixtures, add solvent N-methyl pyrilidone（NMP）, it is prepared into after stirring 2h
Sticky pulpous state electrode material；
（5）By step（4）In obtained sticky pulpous state electrode material, coated on metal copper foil, coating thickness is not more than 50 μm,
Under the conditions of drying temperature is not higher than 120 DEG C, drying time is not less than 6h, obtains lithium ion battery electrode material；
（6）By step（6）In obtained battery electrode material be cut into the circular pole piece that diameter meets the requirement of battery electrode size, gold
Category lithium piece is used as is to electrode, electrolyte：1mol/L LiPF6It is dissolved in ethylene carbonate（EC）And dimethyl carbonate（DMC）'s
In solvent（Mol ratio EC：DMC=1:1）, it is assembled into 2032 type button cells.
2. a kind of preparation method of metal complex lithium ion battery electrode material according to claim 1, its feature exist
In：Mg (the NO3)2·6H2O, N, N- bis- (5- M-phthalic acids)-Isosorbide-5-Nitrae, 5,8- benzene-naphthalene diimides, it is that analysis is pure.
3. a kind of preparation method of metal complex lithium ion battery electrode material according to claim 1 or 2, its feature
It is：Mg (the NO3)2·6H2O adds 5~10mmol to volume as in 50~100mL reactors；(the 5- isophthalic of N- bis-
Dioctyl phthalate)-Isosorbide-5-Nitrae, 5,8- benzene-naphthalene diimides, add 2.5~5mmol；Concentration of hydrochloric acid is 3-6mol/L；Ptfe autoclave
Volume is 50~100mL.
4. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
It is DMF to state solvent, adds 30~60mL to volume as in 50~100mL reactors.
5. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
State step（1）In mixing time be 30~60min, stir speed (S.S.) is 200~500 r/min.
6. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
State step（2）In reaction temperature be 90~100 DEG C；Step（2）Middle constant temperature time is more than 24h.
7. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
State step（3）Middle ethanol exchange reaction, the ratio that ethanol adds is by ethanol weight than crystal weight 10~20:1.
8. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
State step（3）Middle ethanol exchange reaction, ethanol is changed every 6~8h, exchange times are 3~4 times.
9. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：Institute
State step（3）Middle ethanol is filtered after exchanging, and 10~12h is dried in vacuo at 80~100 DEG C.
10. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：
The step（4）Middle complex Mg-NDI, PVDF, Super-P are according to mass ratio 60:10:30 or 50:10:40；What NMP was added
Measure as 3~4 times of complex Mg-NDI, PVDF, Super-P gross weight.
11. the preparation method of metal complex lithium ion battery electrode material according to claim 1, it is characterised in that：
The step（5）Middle electrode slurry coating thickness is that 6~12h is dried at 30~50 μm, 100~120 DEG C.
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| CN108615891A (en) * | 2018-04-18 | 2018-10-02 | 曲靖师范学院 | A kind of preparation method of zinc-base complex lithium ion battery negative material |
| CN108666573A (en) * | 2018-04-23 | 2018-10-16 | 曲靖师范学院 | A kind of preparation method of titanium-based MOF lithium ion battery negative materials |
| CN111359635A (en) * | 2020-04-13 | 2020-07-03 | 新昌县佳和工艺股份有限公司 | Porous carbon material loaded FeCo2S4Electrochemical oxygen evolution catalyst and preparation method thereof |
| CN111446414A (en) * | 2020-04-07 | 2020-07-24 | 曲靖师范学院 | Covalent organic framework material, preparation method and application thereof |
| CN113178550A (en) * | 2021-04-30 | 2021-07-27 | 桂林理工大学 | Aluminum composite electrode, preparation method and application thereof, and dual-ion battery |
| CN113764688A (en) * | 2021-08-27 | 2021-12-07 | 北京工业大学 | Three-dimensional carbon structure supported GaN catalyst and preparation method thereof |
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| CN108615891A (en) * | 2018-04-18 | 2018-10-02 | 曲靖师范学院 | A kind of preparation method of zinc-base complex lithium ion battery negative material |
| CN108615891B (en) * | 2018-04-18 | 2020-06-16 | 曲靖师范学院 | Preparation method of zinc-based complex lithium ion battery negative electrode material |
| CN108666573A (en) * | 2018-04-23 | 2018-10-16 | 曲靖师范学院 | A kind of preparation method of titanium-based MOF lithium ion battery negative materials |
| CN111446414A (en) * | 2020-04-07 | 2020-07-24 | 曲靖师范学院 | Covalent organic framework material, preparation method and application thereof |
| CN111359635A (en) * | 2020-04-13 | 2020-07-03 | 新昌县佳和工艺股份有限公司 | Porous carbon material loaded FeCo2S4Electrochemical oxygen evolution catalyst and preparation method thereof |
| CN111359635B (en) * | 2020-04-13 | 2021-12-14 | 浙江致远环境科技有限公司 | Porous carbon material loaded FeCo2S4Electrochemical oxygen evolution catalyst and preparation method thereof |
| CN113178550A (en) * | 2021-04-30 | 2021-07-27 | 桂林理工大学 | Aluminum composite electrode, preparation method and application thereof, and dual-ion battery |
| CN113764688A (en) * | 2021-08-27 | 2021-12-07 | 北京工业大学 | Three-dimensional carbon structure supported GaN catalyst and preparation method thereof |
| CN113764688B (en) * | 2021-08-27 | 2024-02-06 | 北京工业大学 | Three-dimensional carbon structure supported GaN catalyst and preparation method thereof |
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